WO2018079475A1 - プリプレグ積層体、繊維強化複合材料および繊維強化複合材料の製造方法 - Google Patents

プリプレグ積層体、繊維強化複合材料および繊維強化複合材料の製造方法 Download PDF

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Publication number
WO2018079475A1
WO2018079475A1 PCT/JP2017/038162 JP2017038162W WO2018079475A1 WO 2018079475 A1 WO2018079475 A1 WO 2018079475A1 JP 2017038162 W JP2017038162 W JP 2017038162W WO 2018079475 A1 WO2018079475 A1 WO 2018079475A1
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Prior art keywords
prepreg
fiber
reinforced composite
composite material
resin
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PCT/JP2017/038162
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English (en)
French (fr)
Japanese (ja)
Inventor
畑中和洋
中川教生
▲ヌデ▼島英樹
竹本秀博
Original Assignee
東レ株式会社
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Application filed by 東レ株式会社 filed Critical 東レ株式会社
Priority to KR1020197010515A priority Critical patent/KR102362050B1/ko
Priority to CN201780065056.7A priority patent/CN109952182A/zh
Priority to EP17865288.9A priority patent/EP3533575B1/de
Priority to US16/342,030 priority patent/US11001033B2/en
Priority to JP2017560825A priority patent/JPWO2018079475A1/ja
Publication of WO2018079475A1 publication Critical patent/WO2018079475A1/ja

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Definitions

  • the present invention relates to a fiber reinforced composite material, a method for producing a fiber reinforced composite material, and a prepreg laminate suitably used for the method.
  • Fiber-reinforced composite materials are useful because they are excellent in strength, rigidity, conductivity and the like. Widely deployed in computer applications such as aircraft structural members, windmill blades, automobile exterior materials, automotive interior materials, and IC trays and notebook computer housings, the demand is increasing year by year.
  • the fiber reinforced composite material is a material formed by molding a prepreg having, for example, reinforcing fibers and a resin as essential components.
  • a prepreg having, for example, reinforcing fibers and a resin as essential components.
  • the fiber-reinforced composite material obtained when air or volatile components remain in the resin part of the prepreg before or during molding generates pinholes on the surface and voids inside. ing. Therefore, various techniques have been proposed for the purpose of reducing pinholes and voids inside the fiber-reinforced composite material obtained from the prepreg.
  • a technique has been proposed in which a SMC (Sheet Molding Compound) molding material and a nonwoven fabric not impregnated with resin are press-molded to give a fiber-reinforced composite material (see Patent Document 1).
  • a technique of a fiber reinforced resin molded product in which a fiber mat not impregnated with a resin is laminated between prepreg materials in which a reinforcing fiber is impregnated with a resin such as polypropylene has been proposed (see Patent Document 2). ).
  • the undulation of the fibers due to the fluidity was suppressed, and as a result, the generation of irregularities on the surface of the SMC molded product could be suppressed.
  • it was possible to improve the peel strength of the fiber-reinforced composite material by smoothing the surface of the fiber-reinforced composite material and eliminating the resin-only layer at the time of lamination molding, and strengthening the space between the layers.
  • the desired design could not be obtained even if the surface of the fiber reinforced composite material was designed.
  • the surface of the fiber reinforced composite material that will be designed is referred to as the design surface.
  • JP 2008-246981 A Japanese Patent Laid-Open No. 5-269909
  • An object of the present invention is to provide a carbon fiber reinforced composite material having an excellent design surface.
  • the present invention discloses the following aspects.
  • the following invention is disclosed as a prepreg laminate.
  • (1) including a prepreg [a] in which a reinforcing fiber is impregnated in a reinforcing fiber and a base material [b] in which a resin is not impregnated,
  • the prepreg [a] has a structure in which at least two prepregs [a] are continuously laminated,
  • a prepreg laminate including a structure in which both sides of the substrate [b] are sandwiched by the prepreg [a].
  • the preferred embodiments of the invention include the following.
  • At least one surface of the prepreg laminate is a design surface, and the prepreg [a], the substrate [b], and two or more prepregs [a] are sequentially formed from the outermost layer on the design surface side. Any one of the above prepreg laminates having a laminated structure.
  • prepreg [a2] prepreg [a] laminated on the other surface of the substrate [b] (however, when the prepreg [a] is laminated, a laminate of the prepreg [a]).
  • Prepreg structure [a1] laminated on one surface of the base material [b], comprising the prepreg [a] in which two or more prepregs [a] are continuously laminated. Structure.
  • Preferred embodiments of the above invention include the following.
  • this invention discloses the manufacturing method of the following fiber reinforced composite materials.
  • a method for producing a fiber-reinforced composite material comprising a step of heating and pressurizing any one of the prepreg laminates.
  • the method for producing a fiber-reinforced composite material further comprising a step of performing any one of the molding steps at a pressure of ⁇ 80 kPa or less (gauge pressure).
  • the method for producing any one of the above fiber-reinforced composite materials wherein the resin contained in the prepreg [a] is impregnated into the substrate [b] in the step of heating and pressurizing.
  • a fiber-reinforced composite material having an excellent design surface can be obtained.
  • the prepreg laminate according to the present invention is a prepreg laminate including two or more prepregs [a] in which a resin is impregnated in a reinforcing fiber and one or more base materials [b] in which a resin is not impregnated.
  • the laminate has a structure in which at least two prepregs [a] in which a reinforcing fiber is impregnated with a resin are continuously laminated, and both sides of the substrate [b] are sandwiched by the prepregs [a]. including.
  • the prepreg laminate 10 shown in FIG. 1 has a prepreg [a] disposed on both sides of a base material [b] 3 and sandwiches the base material [b] 3.
  • a prepreg [a] 2a2 On the upper side of the substrate [b] 3, there is a prepreg [a] 2a2 and further there is a prepreg [a] 2a1. In the case of such an adjacent arrangement, it can be said to be “continuously”.
  • the surface of the prepreg [a] 2b1 is the design surface 1.
  • the resin impregnated in the prepreg [a] moves to the base [b] 3 and is impregnated between the fibers contained in the base [b] 3.
  • the prepreg [a] 2a1 and the prepreg [a] 2a2 are laminated in succession to form a base material from these prepregs [a] when a fiber-reinforced composite material is produced by heating and pressing.
  • the resin is impregnated into 3 and the air and volatile components contained in the prepreg [a] are transferred to the substrate [b] 3 together with the resin contained in the prepreg [a] 2b1 having a design surface.
  • a fiber-reinforced composite material having an excellent design surface 1 can be obtained.
  • the prepreg [a] used in the present invention contains at least reinforcing fibers and a resin.
  • Metal fibers such as aluminum fibers, brass fibers, stainless fibers; PAN-based carbon fiber, rayon-based carbon fiber, lignin-based carbon fiber, pitch-based carbon fiber carbon fiber; Graphite fiber; glass fiber; Organic fibers such as aramid fiber, PBO fiber, polyphenylene sulfide fiber, polyester fiber, acrylic fiber, nylon fiber, polyethylene fiber; Inorganic fibers such as silicon carbide fiber and silicon nitride fiber.
  • these fibers may be subjected to a surface treatment.
  • the surface treatment include a treatment with a coupling agent, a treatment with a sizing agent, a treatment with a binding agent, and an adhesion treatment of an additive in addition to a process for depositing a metal as a conductor.
  • These reinforcing fibers may be used alone or in combination of two or more.
  • carbon fibers such as PAN-based carbon fibers, pitch-based carbon fibers, and rayon-based carbon fibers that are excellent in specific strength and specific rigidity are preferably used from the viewpoint of weight reduction effect.
  • a relatively inexpensive glass fiber is preferably used.
  • carbon fiber and glass fiber in combination from the balance of mechanical properties and economy.
  • aramid fibers are also preferably used from the viewpoint of improving the impact absorbability of the resulting fiber-reinforced composite material and the formability of the laminate, and in particular, carbon fibers and aramid fibers are used in combination from the balance of mechanical properties and impact absorbability. It is preferable.
  • reinforcing fibers coated with a metal such as nickel, copper, ytterbium, etc. can be used.
  • a metal such as nickel, copper, ytterbium, etc.
  • PAN-based carbon fibers having excellent mechanical properties such as strength and elastic modulus can be used more preferably.
  • the form of the reinforcing fiber is not limited to a continuous or discontinuous form.
  • the arrangement is not limited as long as it is a continuous form.
  • the reinforcing fibers are preferably in the form of continuous fibers such as long fibers, woven fabrics, tows, and rovings that are aligned in one direction.
  • the fabric structure include plain weave, twill weave, and satin weave.
  • a reinforcing fiber having a fiber length of less than 15 mm is preferable from the viewpoint of easy kneading as a filler.
  • thermosetting resin and a thermoplastic resin are mentioned.
  • thermosetting resin a thermosetting resin such as an epoxy resin, a phenol resin, a vinyl ester resin, a benzoxazine resin, a polyimide resin, an oxetane resin, a maleimide resin, an unsaturated polyester resin, a urea resin, or a melamine resin is preferably used. be able to.
  • a resin in which two or more kinds are blended may be applied.
  • an epoxy resin, a phenol resin, and a vinyl ester resin are preferable from the viewpoint of the mechanical properties and heat resistance of the laminate.
  • an epoxy resin is more preferable from the viewpoint of handling properties in addition to the mechanical properties of the laminate and heat resistance.
  • the epoxy resin is preferably contained as a main component of the resin to be used in order to express its excellent mechanical properties, and specifically, it is preferably contained by 60% by mass or more per resin composition.
  • an epoxy resin having an amine, a phenol, or a compound having a carbon-carbon double bond as a precursor is preferably used.
  • any compound having an active group capable of reacting with an epoxy group can be used.
  • a compound having an amino group, an acid anhydride group and an azide group is suitable.
  • the curing agent include dicyandiamide, various isomers of diaminodiphenylmethane and diaminodiphenylsulfone, aminobenzoic acid esters, various acid anhydrides, phenol novolac resins, cresol novolac resins, polyphenol compounds, imidazole derivatives, aliphatic amines, tetraamines, and the like.
  • Examples include methylguanidine, thiourea addition amine, carboxylic acid anhydride such as methylhexahydrophthalic anhydride, carboxylic acid hydrazide, carboxylic acid amide, polymercaptan, and Lewis acid complex such as boron trifluoride ethylamine complex. . These curing agents may be used alone or in combination.
  • aromatic diamine As a curing agent, a cured resin having good heat resistance can be obtained.
  • various isomers of diaminodiphenylsulfone are most suitable for obtaining a cured resin having good heat resistance.
  • the equivalent ratio in some cases, for example, by setting the equivalent ratio in the vicinity of 0.7 to 0.8, a high elastic modulus can be obtained.
  • the cured resin is obtained.
  • a combination of dicyandiamide and a urea compound such as 3,4-dichlorophenyl-1,1-dimethylurea or imidazoles as a curing agent
  • high heat and water resistance can be obtained while curing at a relatively low temperature. It is done.
  • Curing with an acid anhydride gives a cured resin having a lower water absorption than amine compound curing.
  • a latent product of these curing agents for example, a microencapsulated product can be used.
  • epoxy resin curing agents a combination of dicyandiamide and a urea compound is preferably used because it can be cured within 10 minutes at a temperature of 145 ° C. or higher.
  • composition of the epoxy resin and the curing agent not only the composition of the epoxy resin and the curing agent, but also a product obtained by pre-reacting a part of them can be blended in the composition.
  • This method may be effective for viscosity adjustment and storage stability improvement.
  • thermoplastic resin dissolved in the thermosetting resin.
  • a thermoplastic resin is generally selected from a carbon-carbon bond, an amide bond, an imide bond, an ester bond, an ether bond, a carbonate bond, a urethane bond, a thioether bond, a sulfone bond and a carbonyl bond in the main chain.
  • a thermoplastic resin having a bond is preferable.
  • thermosetting resins include polyamide resins, polycarbonate resins, polyacetal resins, polyphenylene oxide resins, polyphenylene sulfide resins, polyarylate resins, polyester resins, polyamideimide resins, polyimide resins, polyetherimide resins, Polyimide resins having a phenyltrimethylindane structure, polysulfone resins, polyethersulfone resins, polyetherketone resins, polyetheretherketone resins, polyaramide resins, polyethernitrile resins, and polybenzimidazole resins.
  • thermoplastic resin examples include the following. Polyolefin resins such as polyethylene resin, polypropylene resin, polybutylene resin; Polyester resins such as polyethylene terephthalate resin, polybutylene terephthalate resin, polytrimethylene terephthalate resin, polyethylene naphthalate resin, liquid crystal polyester; Polyamide resin, polyoxymethylene resin; polyarylene sulfide resin such as polyphenylene sulfide resin; polyketone resin, polyether ketone resin, polyether ether ketone resin, polyether ketone ketone resin, polyether nitrile resin; polytetrafluoroethylene resin, etc.
  • Polyolefin resins such as polyethylene resin, polypropylene resin, polybutylene resin
  • Polyester resins such as polyethylene terephthalate resin, polybutylene terephthalate resin, polytrimethylene terephthalate resin, polyethylene naphthalate resin, liquid crystal polyester
  • Polyamide resin polyoxymethylene resin
  • Crystalline resins such as fluorinated resins and liquid crystal polymer resins; Amorphous resins such as polystyrene resin, polycarbonate resin, polymethyl methacrylate resin, polyvinyl chloride resin, polyphenylene ether resin, polyimide resin, polyamideimide resin, polyetherimide resin, polysulfone resin, polyethersulfone resin, polyarylate resin ; Thermoplastics such as phenol resin, phenoxy resin, polystyrene resin, polyolefin resin, polyurethane resin, polyester resin, polyamide resin, polybutadiene resin, polyisoprene resin, fluorine resin, and polyacrylonitrile resin Thermoplastic resins selected from elastomers and the like, and copolymers or modified products thereof.
  • Amorphous resins such as polystyrene resin, polycarbonate resin, polymethyl methacrylate resin, polyvinyl chloride resin, polyphenylene ether resin, polyimide resin, poly
  • a polyolefin resin is preferable from the viewpoint of light weight of the obtained laminate
  • a polyamide resin is preferable from the viewpoint of strength
  • a polyester resin is preferably used from the viewpoint of surface appearance.
  • the resin impregnated in the prepreg [a] may further contain an impact resistance improver such as an elastomer or a rubber component, and other fillers and additives as long as the object of the present invention is not impaired.
  • an impact resistance improver such as an elastomer or a rubber component
  • other fillers and additives as long as the object of the present invention is not impaired.
  • these include inorganic fillers, flame retardants, conductivity imparting agents, crystal nucleating agents, ultraviolet absorbers, antioxidants, vibration damping agents, antibacterial agents, insect repellents, deodorants, anti-coloring agents, heat stabilizers. , Release agents, antistatic agents, plasticizers, lubricants, colorants, pigments, dyes, foaming agents, antifoaming agents, or coupling agents.
  • filler calcium carbonate, talc, silica, clay, glass flake, catechin, zeolite, silica balloon, glass balloon, shirasu balloon, carbon black, carbon nanotube, fullerene, graphite, metal powder, metal foil, ferrite material, alumina
  • filler examples thereof include barium titanate, lead zirconate titanate, barium sulfate, titanium oxide, glass beads, alumina, antimony oxide, hydrotalcite, red phosphorus, zinc carbonate, and calcium oxide.
  • an intermediate base material containing continuous reinforcing fibers is preferable from the viewpoint of moldability.
  • the base material [b] used for the prepreg laminate preferably contains fibers because the resin is easily impregnated during molding.
  • fibers that can be used for the substrate [b] include the following.
  • Metal fibers such as aluminum fibers, brass fibers, stainless fibers; PAN-based carbon fiber, rayon-based carbon fiber, lignin-based carbon fiber, pitch-based carbon fiber carbon fiber; graphite fiber, glass fiber; Organic fibers such as aramid fiber, PBO fiber, polyphenylene sulfide fiber, polyester fiber, acrylic fiber, nylon fiber, polyethylene fiber; Inorganic fibers such as silicon carbide fiber and silicon nitride fiber.
  • these fibers may be subjected to a surface treatment.
  • the surface treatment include a treatment with a coupling agent, a treatment with a sizing agent, a treatment with a binding agent, and an adhesion treatment of an additive in addition to a process for depositing a metal as a conductor.
  • these reinforcing fibers may be used individually by 1 type, and may use 2 or more types together.
  • carbon fibers such as PAN-based carbon fibers, pitch-based carbon fibers, and rayon-based carbon fibers that are excellent in specific strength and specific rigidity are preferably used from the viewpoint of weight reduction effect.
  • relatively inexpensive glass fibers are preferably used, and in particular, carbon fibers and glass fibers are preferably used in combination from the balance of mechanical properties and economic efficiency.
  • aramid fibers are preferably used from the viewpoint of improving the impact absorbability of the obtained fiber-reinforced composite material and the formability of the laminate. Furthermore, it is preferable to use a carbon fiber and an aramid fiber in combination from the balance of mechanical properties and impact absorption.
  • reinforcing fibers coated with a metal such as nickel, copper, or ytterbium can also be used.
  • PAN-based carbon fibers excellent in mechanical properties such as strength and elastic modulus, and glass fibers can be used more preferably from the viewpoint of improving the economic efficiency of the resulting laminate.
  • the substrate [b] may be any material that is not impregnated with a resin, and examples of the form include a nonwoven fabric, a woven fabric, a knitted fabric, and a mat. Examples of the fabric structure include plain weave, twill weave, and satin weave.
  • the substrate [b] preferably contains carbon fiber or glass fiber. Further, the fibers are preferably discontinuous. A substrate containing carbon fiber is excellent in strength and elastic modulus, and a substrate containing glass fiber can provide a fiber-reinforced composite material excellent in economic efficiency. It is preferable that the fiber is a discontinuous substrate because the thickness of the substrate can be adjusted in a wide range, and thus the thickness of the resulting fiber-reinforced composite material can be adjusted.
  • the prepreg laminate has a configuration in which at least one surface of the prepreg laminate is the design surface 1 and the base material prepreg [a] is laminated up to the outermost layer on the design surface 1 side and the second or third layer. This is preferable in that pinholes on the design surface of the fiber-reinforced composite material obtained can be suppressed.
  • the prepreg [a] 2 b 1 that becomes the design surface 1 is obtained by forming the prepreg laminate 10 in which the prepreg [a] 2 b 1 and then the base material [b] 3 are arranged from the design surface 1. Air and volatile components are impregnated and moved into the substrate [b] 3 together with the resin. As a result, an excellent design surface of the fiber reinforced composite material can be obtained. That is, the prepreg laminate has at least one surface as a design surface, and two or more prepregs [a], base materials [b], and prepregs [a] are successively formed from the design surface side. Arranging in the order of the laminated structure is preferable in that pinholes on the design surface of the obtained fiber-reinforced composite material are suppressed.
  • the prepreg [a] 2b2 and the prepreg [a] 2b1 are arranged so that the prepreg [a] has two layers. Furthermore, base material [b] 3 can be arrange
  • the prepreg [a] 2a2 and the prepreg [a] 2a1 are further laminated in order on the substrate [b] 3, and the prepreg laminate 10 having a large total number of laminated prepregs [a].
  • the prepreg laminated body 10 of FIG. 4 the prepreg [a] 2a2 and the prepreg [a] 2a1 are arranged in order on one side of the substrate [b] 3, and the prepreg [a] 2b1 and the prepreg [a] 2b2 are sequentially arranged on one side. It has a distributed structure.
  • the basis weight of the substrate [b] used in the prepreg laminate is preferably 5 to 100 g / m 2 .
  • the basis weight of the substrate [b] used in the prepreg laminate is preferably 5 to 100 g / m 2 .
  • the improvement of the moldability of a prepreg laminated body and the designability of a fiber reinforced composite material can be aimed at. More preferably, it is 5 to 80 g / m 2 , further preferably 5 to 50 g / m 2 , and further 5 to 35 g / m 2 .
  • the basis weight When the basis weight is small, there may be many pinholes on the design surface of the fiber-reinforced composite material obtained.
  • the base material [b] When 100 g / m 2 is large, the base material [b] is not sufficiently impregnated with the resin being molded.
  • the resulting fiber reinforced composite material may have problems with mechanical properties.
  • the thickness of the base material [b] included in the prepreg laminate of the present invention is preferably in the range of 0.1 to 1.5 mm.
  • the impregnation property to the base material [b] of resin and the design property of a fiber reinforced composite material can be compatible. More preferably, it is 0.1 to 1 mm, and still more preferably 0.1 to 0.5 mm. If the thickness is less than 0.1 mm, the design surface of the resulting fiber reinforced composite material may have more pinholes, and if it exceeds 1.5 mm, there will be a problem with the mechanical properties of the resulting fiber reinforced composite material. There is.
  • the thickness of the prepreg structure [a1] defined below is preferably 0.2 to 9 times the thickness of one prepreg [a2] defined below.
  • Prepreg structure [a1] laminated on one surface of the base material [b], comprising the prepreg [a] in which two or more prepregs [a] are continuously laminated.
  • Prepreg [a2] Prepreg [a] laminated on the other surface of the substrate [b] (however, when the prepreg [a] is laminated, a laminate of the prepreg [a]). This thickness ratio makes it possible to achieve both the impregnation of the substrate [b] 3 and the design of the fiber-reinforced composite material.
  • the thickness of the substrate [b] is preferably 0.1 to 3.0 times the thickness of the prepreg structure [a1].
  • the impregnation property to base material [b] 3 and the designability of a fiber reinforced composite material can be aimed at. More preferably, it is 0.2 to 2 times, and still more preferably 0.5 to 1 times.
  • the prepreg laminate prepreg [a] can be designed according to the mechanical properties required by the fiber reinforced composite material, the thickness of the fiber reinforced composite material, and the like.
  • the prepreg laminate includes a structure in which two or more prepregs [a] in which a resin is impregnated with a reinforcing fiber is continuously laminated, whereby the resin is changed from the prepreg [a] to the base material [b] by a molding operation. Even after impregnation, the void content is low, resulting in a fiber-reinforced composite material having excellent mechanical properties such as strength.
  • the material has a design surface with few pinholes.
  • the fiber reinforced composite is impregnated into the base material and supplied
  • the fiber volume content of the material increases, and the void content tends to increase.
  • pinholes on the design surface may still occur.
  • a prepreg laminate is obtained by laminating a prepreg in accordance with the mechanical properties, thickness, etc. of the target fiber-reinforced composite material.
  • This fiber reinforced composite material includes a fiber reinforced composite material layer [A] derived from a prepreg [a] in which a reinforced fiber is impregnated with a resin, and a fiber reinforced composite material derived from a base material [b] not impregnated with a resin.
  • the material layer [B] is included.
  • the resin of the prepreg [a] is cured or solidified.
  • the fiber-reinforced composite material layer [B] of the fiber-reinforced composite material of the present invention a part of the resin in the prepreg [a] was impregnated into the base material [b], and the resin was cured or solidified therein. Is.
  • the average fiber volume content of the fiber reinforced composite material layer [A] is VfA and the fiber volume content of the fiber reinforced composite material layer [B] is VfB, VfA> VfB. It is preferable to have a relationship.
  • VfA is preferably 55% or more and VfB is 40% or less from the viewpoint of design of the fiber-reinforced composite material.
  • the resin impregnated in the fiber reinforced composite material layer [B] is the resin impregnated in the prepreg [a].
  • the fiber volume content of the fiber reinforced composite material layer [A] on both sides sandwiching the fiber reinforced composite material layer [A] is preferably 55 to 90%.
  • the mechanical properties and design properties of the fiber-reinforced composite material are excellent.
  • it is 60 to 90%, more preferably 70 to 80%. If the fiber volume content is small, the resin layer contained in the fiber reinforced composite material layer [A] increases, and air and volatile components are difficult to move to the fiber reinforced composite material layer [B], and the design of the fiber reinforced composite material is sufficient. May not be achieved.
  • the fiber volume content of the fiber reinforced composite material layer [B] is preferably 1 to 40% from the viewpoint of the impregnation property of the resin in the prepreg. More preferably, it is 2 to 30%, and further 2 to 10%.
  • the fiber reinforced composite material layer [B] has a void content higher than the average of the void content of each fiber reinforced composite material layer [A]. It is preferable at the point which can improve.
  • the voids of the fiber reinforced composite material layer [B] are distributed in the range of 80 to 100% in the central portion of the fiber reinforced composite material layer [B] on the cut surface along the lamination direction of the prepreg [a] and the base material [b]. It is preferable. This is because the adhesion between the layers is increased in the resulting fiber reinforced composite material.
  • the manufacturing method of the fiber reinforced composite material of this invention has the process of heating and pressurizing the prepreg laminated body demonstrated above, and shape
  • the step of further reducing the pressure is performed in the step of forming the prepreg laminate and the step of impregnating the resin contained in the prepreg [a] into the base material [b] and molding. It is preferable to include. This is because the resulting fiber-reinforced composite material is excellent in design. By reducing the pressure, air and volatile components remaining near the design surface of the prepreg laminate are removed. As a result, a fiber-reinforced composite material having a more excellent design surface can be obtained.
  • Under reduced pressure is a pressure of ⁇ 80 kPa or less, preferably ⁇ 90 kPa or less, more preferably ⁇ 95 kPa or less in terms of gauge pressure.
  • Examples of the method for producing the fiber-reinforced composite material of the present invention include press molding using a mold, vacuum bag molding, autoclave molding, and the like. Among these, the production method by autoclave molding is preferable because a fiber-reinforced composite material having an excellent design surface can be obtained.
  • the molding pressure in autoclave molding is preferably from 0.1 MPa to 1.0 MPa, and more preferably from 0.3 MPa to 0.6 MPa from the viewpoint that pinholes on the design surface can be removed.
  • the molding temperature in autoclave molding needs to be set according to the curing temperature of the resin used in the prepreg, but is usually in the range of 100 ° C to 200 ° C.
  • the coating surface of the obtained fiber reinforced composite material is subjected to painting treatment such as clear painting and colored painting, and film pasting. Since the fiber-reinforced composite material has a design surface with few pinholes, the effect of the present invention is remarkably exhibited in the present invention.
  • Examples of uses of the fiber-reinforced composite material of the present invention include the following.
  • PC personal digital assistant
  • PDA personal digital assistant such as electronic notebook
  • video camera digital video camera
  • optical equipment audio
  • Electrical and electronic equipment parts such as casings, trays, chassis, interior members, and cases of air conditioners, lighting equipment, entertainment goods, toy goods, and other household appliances.
  • Civil engineering and building material parts such as columns, panels and reinforcements.
  • Suspension, accelerator, or steering components such as various members, various frames, various hinges, various arms, various axles, various wheel bearings, various beams, propeller shafts, wheels, gearboxes, etc.
  • Alternator terminal Alternator terminal, alternator connector, IC regulator, light potentiometer base, engine coolant joint, air conditioning thermostat base, heating / air flow control valve, radiator motor brush holder, turbine vane, wiper motor related parts, distribution Starter switch, starter relay, window washer nozzle, air conditioner panel switch board, coil for fuel related electromagnetic valve, battery tray, AT bracket, head lamp support, pedal housing, protector, horn terminal, step motor rotor, lamp socket, lamp Reflector, lamp housing, brake piston, noise shield, spare tire cover , Solenoid bobbin, engine oil filter, ignition device case, scuff plates, various parts for automobiles and motorcycles, such as fascia.
  • Landing gear pods Landing gear pods, winglets, spoilers, edges, ladders, elevators, failings, ribs, and other aircraft parts.
  • dicyandiamide curing agent, DICY-7, manufactured by Mitsubishi Chemical Corporation
  • DCMU99 3- (3,4-dichlorophenyl) -1,1-dimethyl, which is a curing auxiliary agent
  • An epoxy resin composition was prepared by kneading 3 parts by mass of urea and a curing accelerator (manufactured by Hodogaya Chemical Co., Ltd.).
  • Carbon fiber A A carbon fiber having a total number of filaments of 3,000, a specific gravity of 1.8, a strand tensile strength of 3.5 GPa, and a strand tensile modulus of 230 GPa is spun and sintered with a copolymer of 99 mol% of acrylonitrile and 1 mol% of itaconic acid. Got. Subsequently, the carbon fiber was subjected to an electrolytic surface treatment using an aqueous sulfuric acid solution having a concentration of 0.05 mol / L as an electrolyte and an electric quantity of 3 coulomb per gram of carbon fiber.
  • the carbon fiber subjected to the electrolytic surface treatment was subsequently washed with water and dried in heated air at a temperature of 150 ° C. to obtain a carbon fiber as a raw material.
  • “jER (registered trademark)” 825 manufactured by Japan Epoxy Resin Co., Ltd.
  • acetone was mixed with acetone to obtain an approximately 1% by mass acetone solution which was uniformly dissolved.
  • heat treatment was performed at a temperature of 210 ° C. for 180 seconds to obtain a sizing agent-coated carbon fiber.
  • the adhesion amount of the sizing agent was adjusted to 0.5 parts by mass with respect to 100 parts by mass of the surface-treated carbon fiber.
  • the prepared epoxy resin composition was applied onto release paper using a knife coater to produce two 66 g / m 2 resin films.
  • a carbon fiber sheet A having a basis weight of 198 g / m 2 in which the resin film obtained as described above was arranged in a twilled two-way cloth in a sheet form, was prepared.
  • the two resin films produced above are stacked from both sides of the carbon fiber sheet A, and impregnated with resin by heating and pressing.
  • the mass fraction of the matrix resin is 40.0%
  • the basis weight is 330 g / m 2
  • the thickness is 0.
  • a 22 mm cross prepreg was prepared.
  • Base material A “Torayca (registered trademark)” Cross CO6151B (manufactured by Toray Industries, Inc.) (weight per unit: 92 g / m 2 , thickness: 0.11 mm)
  • Base material B “Torayca (registered trademark)” Cross CO6343B (manufactured by Toray Industries, Inc.)) (weight per unit area: 198 g / m 2 , thickness: 0.25 mm)
  • Substrate C Surface mat, FC-30S (manufactured by Central Glass Fiber Co., Ltd.) (weight per unit: 30 g / m 2 , thickness: 0.23 mm)
  • Fiber reinforced composite material layer [A] and fiber reinforced composite material layer [B] fiber volume content in the fiber reinforced composite material From the fiber reinforced composite material obtained in each example, in a plane perpendicular to the stacking direction In the direction, a sample 20 mm long x 20 mm wide was cut out, the cross section was polished, the cross section was magnified 200 times or more with a laser microscope (KEYENCE VK-9510), and a photograph was taken so as to fit in the field of view of two or more layers. did. From the same operation, 10 points were randomly selected for each layer, and the thickness of each layer was measured. The fiber volume content of each layer was determined from the thickness of each layer, fiber basis weight and fiber specific gravity.
  • the average value of the fiber volume content of the fiber reinforced composite material layer [A] of the sample and the average value of the fiber reinforced composite material layer [B] were obtained. This was performed with a total of 6 samples, and the average value of the 6 samples was defined as the fiber volume content.
  • prepreg A is used as the material of prepreg [a]
  • base material A is used as the base material [b].
  • prepreg A, base material A, first prepreg A and second prepreg A are used.
  • Four layers were laminated in the order of prepreg A to prepare a prepreg laminate.
  • the prepreg A on the design surface corresponds to the prepreg structure [a2] in the present invention
  • the laminated structure composed of the first prepreg A and the second prepreg A corresponds to the prepreg [a1] structure.
  • Examples 2 and 3 A prepreg laminate was produced in the same manner as in Example 1 except that the material of the substrate [b] was changed to that shown in Table 1. The measurement results of the prepared prepreg laminate are shown in Table 1. (Examples 4 to 6) A prepreg composed of a plurality of prepregs A and base materials A in the order shown in Table 1 from the design surface, using prepreg A as the material of prepreg [a] and base material A as the base material [b]. A laminate was produced. The measurement results are shown in Table 1.
  • the fiber-reinforced composite material of the present invention has an excellent design surface. This is because air and volatile components that cause pinholes on the design surface when the resin is impregnated from the prepreg into the non-impregnated base material also move to the non-impregnated base material. Further, since the fiber-reinforced composite material of the present invention has a low void content, it can be expected to have excellent mechanical properties.
  • a fiber-reinforced composite material having an excellent design surface can be obtained, sports equipment such as tennis rackets and golf shafts, automotive exterior materials such as bumpers and doors, automobiles such as chassis and front side members, etc. It is useful because it can be widely used for structural materials or computer applications such as automobile interior materials such as steering and meter visor, aircraft structural members, windmill blades or IC trays and housings of notebook personal computers.
  • Design surface 2 Group 2a1, 2a2, 2a3, 2b1, and 2b2 of prepreg [a]: Prepreg [a] 3: Substrate [b] 10: Prepreg laminate

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PCT/JP2017/038162 2016-10-26 2017-10-23 プリプレグ積層体、繊維強化複合材料および繊維強化複合材料の製造方法 WO2018079475A1 (ja)

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EP3533575A1 (de) 2019-09-04
KR102362050B1 (ko) 2022-02-11
JPWO2018079475A1 (ja) 2019-09-19
US11001033B2 (en) 2021-05-11
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US20190248107A1 (en) 2019-08-15
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